US2577786A - Carbon bisulfide retort - Google Patents
Carbon bisulfide retort Download PDFInfo
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- US2577786A US2577786A US162693A US16269350A US2577786A US 2577786 A US2577786 A US 2577786A US 162693 A US162693 A US 162693A US 16269350 A US16269350 A US 16269350A US 2577786 A US2577786 A US 2577786A
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- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 title claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 132
- 229910052799 carbon Inorganic materials 0.000 claims description 132
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 102
- 229910052717 sulfur Inorganic materials 0.000 claims description 90
- 239000011593 sulfur Substances 0.000 claims description 90
- 238000006243 chemical reaction Methods 0.000 claims description 74
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000000284 resting effect Effects 0.000 claims description 8
- 229960005349 sulfur Drugs 0.000 description 84
- 235000001508 sulfur Nutrition 0.000 description 83
- 239000002245 particle Substances 0.000 description 21
- 239000003610 charcoal Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 229910001018 Cast iron Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 241000837181 Andina Species 0.000 description 1
- 241000283715 Damaliscus lunatus Species 0.000 description 1
- 101100400378 Mus musculus Marveld2 gene Proteins 0.000 description 1
- 241000283984 Rodentia Species 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 229940020445 flector Drugs 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- APVPOHHVBBYQAV-UHFFFAOYSA-N n-(4-aminophenyl)sulfonyloctadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NS(=O)(=O)C1=CC=C(N)C=C1 APVPOHHVBBYQAV-UHFFFAOYSA-N 0.000 description 1
- HYWYRSMBCFDLJT-UHFFFAOYSA-N nimesulide Chemical compound CS(=O)(=O)NC1=CC=C([N+]([O-])=O)C=C1OC1=CC=CC=C1 HYWYRSMBCFDLJT-UHFFFAOYSA-N 0.000 description 1
- 229960000965 nimesulide Drugs 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
Definitions
- This invention relates to an improved apparatus or retort useful in the manufacture of carbon bisulde.
- Carbon bisulfide is commonly produced by the reaction of carbon and sulfur; the term carbon is employed generically herein as referring to any solid carbon source suitable for reaction with sulfur such as charcoal, coke, coal or other carbon, as is mentioned in U. S. Patent 2,036,840, or a specially prepared carbon such as that of U. S. Patent 1,709,611.
- the reaction is usually conducted in a vertical tubular vshell or retort, the sulfur being introduced as Va liquid at the bottom of the shell, While the carbon is fed in at the upper end Vof the vertical shell to maintain the vessel'substanti'aily completely vfilled from the bottom to 'the top.
- the retort 'shell is heated by an yexternally fired fur naceY to raise the temperature of the carbon and sulfur present in the retort to 'that temperature whereat carbon bisulfide is formed; an apparatus typical of that employed is shown in United States Patent No. 321,661.
- Such retorts are subject to numerous failings and objections.
- the Voverall thermal eiciency is relatively low inasmuch as the heat input to the carbon mass and the sulfur is through the wall of the retort and the mass of relatively non-conductive carbon nlling the retort; thetemperature of the furnace must, therefore, be considerably higher than that' required for the reaction.
- the necessity of utilizing considerable excess fuel s inherent in the operation is relatively short, the inorganic salts, ashforming constituents, carbon and sulfur forming incrustations or clinkers on the metal sidewalls of the retort.
- a relatively simple retort for' the reaction of solid carbon and sul-fur is ffectiv'e to heat all the sulfur in the absence of carbon to a uniform temperature for subsequent contact and reactionwith ⁇ carbon in a separate zone in the retort which is'isolated from the' sulfur heating zone.
- a retort is conveniently provided by a functionally unitariT tubular vessel adapted to be positioned vertically ina suitable' furnace; means are provided for feeding sulfur as a liquid or vapor at the bottom of the shell and for introducing solid carbon particles into" an upper portion of the shell.
- the support divides' the'v unitary, tubular vessel into two separate functional units, a re' action zone which is ijllled with carbon vand a heating zone wherein the sulfur is' heated5 to reV action temperature or nearly so.
- the reaction zone is preferably so provided that the heat of reaction can be conserved and used to heat the' carbon and sulfur to a" substantially highertem perature to achieve a maximum rate of reaction.
- the support means for the carbon charge is such that, when it is desired to clean the reaction space in the shell, the carbon and ash remaining on the support means can be released into the lower region of the retort from which they can be readily removed. Since the carbon charge is relatively small and is of materially reduced extent with respect to the charge present in the usual retort, it should be obvious that the hazard of loss of charcoal is materially reduced as is the time required for cleaning. When the reaction zone is clean, the carbon support is replaced ,and a fresh carbon charge placed in the reaction zone.
- the sulfur is heated by radiation, convection and conduction in an unobstructed space dened by a furnace heated wall, the sulfur temperature can be controlled at a definite level by regulating the furnace temperature.
- the reaction Zone can be defined by any one of the materials which are resistant to attack by the reactants. Since heat input to the reaction zone is not necessary, one can use various nonmetallic materials which are corrosion resistant but which are poor heat conductors. In fact, it isA preferred to operate the reaction zone without heat loss so insulation of the reaction Zone is desirable to insure that the heat liberated in the reaction is employed to heat the carbon and sulfur and promote the reaction at temperatures of the order of l100 C.
- Another object of the present invention is to provide an improved carbon bisulde retort in which the sulfur is heated separately to reaction temperature in the retort and is then passed-to the carbon to react therewith.
- the invention includes other objects and features of advantage, some of which, together with the foregoing, Will appear hereinafter wherein the present preferred form of carbon bisuliide retort of this invention is disclosed.
- Figure 1 is a side elevation partly in section, showing a retort in position in a furnace, the latter being shown schematically to simplify illustration.
- Figure 2 is a section taken along line 2-2 of Figure 1.
- Figure 3 is a section taken transversely of a modified form of retort and showing another form of support for the charcoal charge.
- Figure 4 is a section taken along the line of Figure 3.
- Figure 5 is a side elevation partly in section through a modified form of retort embodying the invention.
- FIGS. 6 and 7 are respectively sections taken through the device shown in Figure 5 along the line G--B and line E-'l, each View being on a reduced scale for convenience n illustration.
- the installation includes a suitable furnace structure 6 supplied with heat from a suitable source (not shown).
- Retort l is supported in the furnace 6 and comprises a tubular shell 8 having a bottom closure 9 thereon, the latter usually resting upon the bottom of the furnace.
- the retort is made of any suitable material as cast iron, and is fabricated in any desired manner and of any desired number of parts or sections to provide a functionally unitary shell structure.
- a sulfur inlet l0 is provided in the lower portion of the shell 8 through which sulfur is admitted and ash is removed periodically; a suitable boot I I is connected to the sulfur inlet and extends to the outside of the furnace to permit of feeding of sulfur as liquid or vapor and removal of ash and unused carbon from the bottom of the furnace during cleaning o f the reaction zone.
- each extension I4 includes a vertical riser portion IB of smaller extent, the latter acting as a quid, as will presently appear, for a carbon charge support generally indicated at I1.
- This support includes an annulus I8 having a central cap I9 and an outer annular sulfur vapor def-lector and carbon support 2
- A-rod 22 is secured to the cap i9 to lower the cap into place and to raise it to permit ash and carbon to drop into the sulfur heating zone.
- includes several slots 24 in that portion of the de- Y flector which rests on annulus I8 to permit sulfur Vapor to pass freely into the supported carbon charge.
- Annulus IB is supported on the four extensions I4 in spaced relation to the furnace sidewall by vertical guides I6.
- An end bell structure 26 ( Figures 1-5) rests upon the flange l2 of the retort shell and is provided with a carbon bisulde outlet 21 and a carbon charge inlet 23 closed by a suitable means (not shown) such as a star-feeder or a suitable removable closure plate, as is shown in Figure 5.
- a suitable means such as a star-feeder or a suitable removable closure plate, as is shown in Figure 5.
- the carbon charge support divides the retort generally into two zones, a reaction zone and a sulfur heating zone.
- the reaction zone space is of relatively small extent since at the higher temperatures achievable through concentration and conservation of exothermic heat of reaction, substantialy shorter contact times and higher space velocities are suicient to obtain the desired percentage con- Version.
- the sulfur heating Zone should be sufcient to supply sulfur'vapor at reaction temperature directly to the reaction zone.
- the maximum permissible sulfur feed rate since if this be exceeded, sulfur appears in an undue quantity in the exit gas and the carbon bisulde production rate will decrease.
- the sulfur superheatin'g section* should h'avefsuc'h anarea and coniiguration that, for agi'ven effective furnace' temperature, the sulfur 'is raised to reaction teinpeiaturefThus, if the sulfur ⁇ be admitted as a. vapor at 450 C., then it vis neces- 'sary to yraise it some 350"r C., to 800 C.
- VHeat transmission to the sulfur vapor in the retort can be improved by utilizing iins, Vbaffles o r other internal surface which will absorb radiant ⁇ heat Vand provideadditional heated surface foi" con ⁇ tact with sulfur vapor in the sulfur heating section of the retort.
- the inlet 28 is 'exposed' and rod 22 is 4raised to remove cap i9 from the annulus i8.
- the ash thefnfdrops into lthe sulfur heating zone from which it is readily 'removed through the sulfur feed inlet.
- the cap 'I9 lis thenlowered into position and a freshcarbon charge'in'serted. The retort'is then -ready for further operation.
- the space ⁇ ab is shown as including'a refractory liniigiBS;
- the retort is provided with a plurality of #lugs 6I Y'at 'an elevation in "the tubular shell 4'8 iii's't above the sulfur inlet.
- Supported upon the lugs is a tubular shell 62 lhaving ⁇ several inwardly ex'- tending arms 53 'formed thereonfto rest upon each of the lugs i.
- the shell SZ-fand 'the shell '8 are "preferably cylindrical in shape fand cbncen# tric'ally positioned to provide a sulfur passage 'of uniform sectional size through which the sul-ful' ascends.
- the tubular shell 62 is provided with a conical upper 'end 6B.
- the shell 62 acts as a black -body or heat radiator in the upper portion of' thev tubular shell 8, to heat the sulfur passing between it and the 'shell 8 vby radiation whereby the sulfuris'raisd quien-lf.' toa reaction temperature.
- the upper portion of the shell 3 and end "bell structure v26 includessuitabie refractory linings such asare indicated at "H and 12; that at 12 is particularly 'designed to be resistant to the car# bon-sulfur reaction because reaction 'occurs 'in this region, that is Where Vthe hot sulfur comes into contact with the carbon mass.
- Bell Y28 is preferably provided 'with a ange 'I3 at its upper end from which a tubular member 'i4' depends' in a spaced'relation to the heat refracting vlining nowadays to provide a passage to outlet 2,1 'so that'the carbon in the tubular member is out of the pathof the reaction products. Carbon is added through opening 15 upon raising of cover Tl With lever "This is a continuation-impart of my applicationv Serial N0. 40,512 filed July 24, 1948,' Anotti' abandoned. 5
- Apparatus for the manufacture of'carbon bisuliirieN comprising a furnace; an elongated tubular shellstandi'ng vertically in'said furnace andhaving a first inlet for feeding sulfur intoa lower portion of the vertical shell anda'second inlet for feeding carbon "into an upperpo'rtion of the vertical Shell; 'ra dical abutments intermediate the endso the shell; and s'upportmea'ns'resting on said abutment's and' extending transversely of the ⁇ shell and providing a support forv carbon fed into the shell KAthro'ughsaid second inlet, said support means dividing'th'e shell linto an upper reaction zone wherein'carbon and sulfur 'react and a' lower lzone wherein sulfurv admittedy tofgthe f lower' portion ofthel zo'ne is hea'jted to'a terni perature whereat the sulfur reacts withtle carbony to form carbonbisui
- said outlet being from said upper reaction zone i and communicating with the upper portion of said shell above said support means; said shell beingpositioned in said furnace with at least that portion of the shell defining the sulfur heating zone confined within and receiving heat from the furnace; and a refractory lining in said shell in that portion of the shell providing said reaction zone.
- Apparatus for the manufacture of carbon bisulde comprising a furnace; an elongated l tubular shell standing vertically in said furnace and having a first inlet for feeding sulfur into a lower portion of the vertical shell and a second inlet for feeding carbon into an upper portion of..
- Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace,
- Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace, a first iniet for feeding sulfur into a lower portion of the vertical shell, a second inlet for feeding vsolid carbon particles into an upper portion n of the vertical shell to provide a mass of carbon particles therein, an outlet from the upper portion of the shell for products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell to divide the shell into an upper reaction zone containing said mass of carbon particles and wherein sulfur vapor and carbon react to form CS2 and leave a solid ash residue and a lower zone which is heated by the furnace and wherein sulfur admitted through said first inlet is heated to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisuliide; said support means including a iirsi-l carbon mass support including an annular grating shelf extending inwardly and transversely of the shell
- Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace, a first inlet for feeding sulfur into a lower portion of the vertical shell in said furnace, a second inlet for feeding solid carbon particles into an upper portion of the vertical shell above said furnace to provide a mass of carbon particles therein, an outlet from the upper portion of the shellfor products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell at an elevation to divide the shell into.
- said support means including carbon mass support including an annular grating shelf extending transversely of the shelf and having an opening therein through which the mass of carbon particles and any ash residue can pass to the lower zone, and at least one frangible support positioned on the grating shelf of said carbon mass support and extending across said opening normally to restrict said opening suciently to retain the mass of carbon particles and the ash residue in the upper zone and admit freely sulfur from the lower zone into contact with the mass of carbon in the upper zone, said frangible support being adapted to be broken with a poker extended down through said reaction zone to release the carbon charge and ash residue into the lower portion of the furnace for removal therefrom.
- Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace to receive heat therefrom in a lower portion, a rst inlet for feeding sulfur into a lower portion of the vertical shell, a second inlet for feeding solid carbon particles into an upper portion of the vertical shell to provide a mass of carbon particles therein, an outlet from the upper portion of the shell for products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell at an elevation to divide the shell into an upper reaction zone containing said massV of carbon particles and wherein sulfur and carbon react to form 10 carbon bisulde and leave an ash residue and a lower zone wherein sulfur admitted through said rst inlet is heated as a vapor to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisulde; said support means including carbon mass support including an annular grating shelf extending transversely of the shell and having an opening there
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Description
Dec. ll, 1951 l. c. MAcDouGALI. 2,577,785
CARBON BISULFIDE RETORT Filed May 1a, 195o 2 SHEETS- SHEET 1 rl Il IN V EN TOR.
Dec. 11, 1951 l. c. MAcDoUGALL CARBON BISULFIYDE RETORT 2 SHEETS-SHEET 2 Filed May 18, 1950 INVENTOR. Iver C. Macdouga/l ATTo/eA/E D ms Patented Dec. 11, 1951 CARBON BISULFIDE RETORT Iver C. Macdougall, Bronxville, N. Y., assigner to Stauiier Chemical Company, a corporation of California Application May 18, 1950, Serial N0. 162,693
7 Claims.
This invention relates to an improved apparatus or retort useful in the manufacture of carbon bisulde. Carbon bisulfide is commonly produced by the reaction of carbon and sulfur; the term carbon is employed generically herein as referring to any solid carbon source suitable for reaction with sulfur such as charcoal, coke, coal or other carbon, as is mentioned in U. S. Patent 2,036,840, or a specially prepared carbon such as that of U. S. Patent 1,709,611.
The reaction is usually conducted in a vertical tubular vshell or retort, the sulfur being introduced as Va liquid at the bottom of the shell, While the carbon is fed in at the upper end Vof the vertical shell to maintain the vessel'substanti'aily completely vfilled from the bottom to 'the top. The retort 'shell is heated by an yexternally fired fur naceY to raise the temperature of the carbon and sulfur present in the retort to 'that temperature whereat carbon bisulfide is formed; an apparatus typical of that employed is shown in United States Patent No. 321,661. Such retorts are subject to numerous failings and objections. For example, the Voverall thermal eiciency is relatively low inasmuch as the heat input to the carbon mass and the sulfur is through the wall of the retort and the mass of relatively non-conductive carbon nlling the retort; thetemperature of the furnace must, therefore, be considerably higher than that' required for the reaction. As a result, the necessity of utilizing considerable excess fuel s inherent in the operation. Also, the life of the retort is relatively short, the inorganic salts, ashforming constituents, carbon and sulfur forming incrustations or clinkers on the metal sidewalls of the retort. These have two objectionable etiects:v They result in a reduction in the rato of heat transmission through the retort wall and so raise i'tste'mperature to one higherY thanthat required fo'r the reaction and wher-eat the attack on the metal is accelerated; They apparently have a deleterious effecten the metal as such for reasons which are' not fully apparent.4 For these reasonsit is usual to replace present retorts after ak period of' operation which is so short relatively that the period is measured' in months. This relatively short retort life is due` to the fact that the reaction` between solidv carbon and sulfur is exothermic and in a conventional retort temperaturesmay belocally' present which are several-hundreddegrees higher than the furnace temperature and which are o f the order' of 1100 C; example, I have actually measured local- 'at 1110o4 C; `and whichiexceeded theofurnace tem- Sil' izedreaction temperatures of lcarbonand sulfur 2 perature by 200 C. At such an elevated teinperature, sulfur will attack the metal retort shell muchy more rapidly than at 800900 C., the teni-- perature necessary to initiate the CS2' reaction.
Because the conventional furnace is filled with charcoal (a poor conductor), the rate of heat transfer to the mass of charcoal and to the sulfur passing through the charcoal is relatively poor, with the result that the production rate Aper unit Vof retort capacity is relatively low; sulfur traversing the central core of charcoal in the re-y tort may even pass through without ever attain# ing reaction temperature. Also, due to the ash and carbon which attach themselves to the re-A tort wall over the life of the retort, Vthe lheating rate falls olf materially as the retort ages with anattendant reduction in production of carbon bisulfide.
In accordance with the present inveinzen,A there is provided a relatively simple retort for' the reaction of solid carbon and sul-fur is ffectiv'e to heat all the sulfur in the absence of carbon to a uniform temperature for subsequent contact and reactionwith `carbon in a separate zone in the retort which is'isolated from the' sulfur heating zone. Such a retort is conveniently provided by a functionally unitariT tubular vessel adapted to be positioned vertically ina suitable' furnace; means are provided for feeding sulfur as a liquid or vapor at the bottom of the shell and for introducing solid carbon particles into" an upper portion of the shell. intermediate the ends of the shell is providedra support upon which the charge of carbon rests in spaced rela# i tion to the lower portion ofv the shell so that the space below the charge support is free of carbon and serves only as a superheater for thelsu-lfur. Thus, the support divides' the'v unitary, tubular vessel into two separate functional units, a re' action zone which is ijllled with carbon vand a heating zone wherein the sulfur is' heated5 to reV action temperature or nearly so. The reaction zone is preferably so provided that the heat of reaction can be conserved and used to heat the' carbon and sulfur to a" substantially highertem perature to achieve a maximum rate of reaction.
To simplify heat insulation problems, it is pre'' erred that the region wherein therreactionl occurs be within the furnace proper, although no heat input is requiredI to the reactionzone'; such" positioning `of' theV reaction z'one` isvno't' necessary and the actual reaction zonecan be outside thev furnace; providing' it is' suitably" heat' in: sulatedA so" thatv the'v reaction proeedsfwithout' heat lossto the atmosphere, utilization" being made of the superheat imparted to the sulfur vapor and of the heat liberated upon the reaction between carbon and the sulfur to increase its reaction rate.
The support means for the carbon charge is such that, when it is desired to clean the reaction space in the shell, the carbon and ash remaining on the support means can be released into the lower region of the retort from which they can be readily removed. Since the carbon charge is relatively small and is of materially reduced extent with respect to the charge present in the usual retort, it should be obvious that the hazard of loss of charcoal is materially reduced as is the time required for cleaning. When the reaction zone is clean, the carbon support is replaced ,and a fresh carbon charge placed in the reaction zone.
-Such 'a retort as I have broadly described possesses many advantages as compared to those which 'have been heretofore employed or proposed. For example, the sulfur is heated by radiation, convection and conduction in an unobstructed space dened by a furnace heated wall, the sulfur temperature can be controlled at a definite level by regulating the furnace temperature. When the sulfur is brought into contact with the carbon, it is at reaction temperature and further heat addition is unnecessary; therefore, the reaction Zone can be defined by any one of the materials which are resistant to attack by the reactants. Since heat input to the reaction zone is not necessary, one can use various nonmetallic materials which are corrosion resistant but which are poor heat conductors. In fact, it isA preferred to operate the reaction zone without heat loss so insulation of the reaction Zone is desirable to insure that the heat liberated in the reaction is employed to heat the carbon and sulfur and promote the reaction at temperatures of the order of l100 C.
It is in general the broad object of the present invention to provide an improved retort for the manufacture of carbon bisulfide.
Another object of the present invention is to provide an improved carbon bisulde retort in which the sulfur is heated separately to reaction temperature in the retort and is then passed-to the carbon to react therewith. l
The invention includes other objects and features of advantage, some of which, together with the foregoing, Will appear hereinafter wherein the present preferred form of carbon bisuliide retort of this invention is disclosed.
In the drawing accompanying and forming a part hereof,
Figure 1 is a side elevation partly in section, showing a retort in position in a furnace, the latter being shown schematically to simplify illustration.
Figure 2 is a section taken along line 2-2 of Figure 1.
Figure 3 is a section taken transversely of a modified form of retort and showing another form of support for the charcoal charge.
, Figure 4 is a section taken along the line of Figure 3.
Figure 5 is a side elevation partly in section through a modified form of retort embodying the invention.
p Figures 6 and 7 are respectively sections taken through the device shown in Figure 5 along the line G--B and line E-'l, each View being on a reduced scale for convenience n illustration.
Referring to thevdrawing, and particularly to Figures 1 and 2, the installation includes a suitable furnace structure 6 supplied with heat from a suitable source (not shown). Retort l is supported in the furnace 6 and comprises a tubular shell 8 having a bottom closure 9 thereon, the latter usually resting upon the bottom of the furnace. The retort is made of any suitable material as cast iron, and is fabricated in any desired manner and of any desired number of parts or sections to provide a functionally unitary shell structure. A sulfur inlet l0 is provided in the lower portion of the shell 8 through which sulfur is admitted and ash is removed periodically; a suitable boot I I is connected to the sulfur inlet and extends to the outside of the furnace to permit of feeding of sulfur as liquid or vapor and removal of ash and unused carbon from the bottom of the furnace during cleaning o f the reaction zone.
Intermediate the ends of the shell 8 are provided a plurality of radial extensions I4, extending inwardly of the shell and spaced about the periphery of the shell. Each extension I4 includes a vertical riser portion IB of smaller extent, the latter acting as a quid, as will presently appear, for a carbon charge support generally indicated at I1. This support includes an annulus I8 having a central cap I9 and an outer annular sulfur vapor def-lector and carbon support 2| secured to the annulus I8. A-rod 22 is secured to the cap i9 to lower the cap into place and to raise it to permit ash and carbon to drop into the sulfur heating zone. `Deflector 2| includes several slots 24 in that portion of the de- Y flector which rests on annulus I8 to permit sulfur Vapor to pass freely into the supported carbon charge. Annulus IB is supported on the four extensions I4 in spaced relation to the furnace sidewall by vertical guides I6.
An end bell structure 26 (Figures 1-5) rests upon the flange l2 of the retort shell and is provided with a carbon bisulde outlet 21 and a carbon charge inlet 23 closed by a suitable means (not shown) such as a star-feeder or a suitable removable closure plate, as is shown in Figure 5.
It will be observed that the carbon charge support divides the retort generally into two zones, a reaction zone and a sulfur heating zone. The reaction zone space is of relatively small extent since at the higher temperatures achievable through concentration and conservation of exothermic heat of reaction, substantialy shorter contact times and higher space velocities are suicient to obtain the desired percentage con- Version. One can feed the carbon continuously or intermittently so long as an adequate charge is present for reaction with the sulfur at any instant.
The sulfur heating Zone should be sufcient to supply sulfur'vapor at reaction temperature directly to the reaction zone. In any given retort, one can determine, for a given furnace temperature, the maximum permissible sulfur feed rate, since if this be exceeded, sulfur appears in an undue quantity in the exit gas and the carbon bisulde production rate will decrease.
By having the sulfur heating section feeding superheated sulfur directly and immediately to the reaction zone, one avoids any heat loss from the sulfur, as inevitably would occur if superheating` and reacting vessels were employed, connected by a conduit. Further, and what is more importantI have found that the superheated sulfur does notY give rise to any corrosion problem in the superheating Zone in the absence vof charcoal or ash. Thus, I l,am able to employ cast iron retorts 'successfully-"to produce' 'more' carbonrbil sulide per unit of retort volume and'atthefsame time, increase materially the usefulretort life. The sulfur superheatin'g section* should h'avefsuc'h anarea and coniiguration that, for agi'ven effective furnace' temperature, the sulfur 'is raised to reaction teinpeiaturefThus, if the sulfur `be admitted as a. vapor at 450 C., then it vis neces- 'sary to yraise it some 350"r C., to 800 C. VHeat transmission to the sulfur vapor in the retort can be improved by utilizing iins, Vbaffles o r other internal surface which will absorb radiant` heat Vand provideadditional heated surface foi" con` tact with sulfur vapor in the sulfur heating section of the retort. A
operation,sulfur is introduced into the sulf ur inlet 10, 'preferably ,as a vapor; the vapor rises through the lower lportion o f the retor'tfand thence into the carbon charge'y in the reaction zron'e. With the furnace operating at a tempera-l ture of between about 800 and 950C., and with the sulfur feed rate commensurate with thefsize of the apparatus, it will be found that the sulfur entering the carbon charge is at'rea'ct'on ternperature, 'e'. g. greater than *750 C., one Whereat the Ereaction between the carbon and sulfur goes on exothermically.
When ashl has accumulated inthe reaction zone to an'undesirable extent, the inlet 28 is 'exposed' and rod 22 is 4raised to remove cap i9 from the annulus i8. The ash thefnfdrops into lthe sulfur heating zone from which it is readily 'removed through the sulfur feed inlet. The cap 'I9 lis thenlowered into position and a freshcarbon charge'in'serted. The retort'is then -ready for further operation.
In' Figures'S and 4, I have shown a modied form of retort in which carbon charge support l1,"the carbon charge andthe reaction zone are outside thefurnace; To'avoid heat loss from the reaction zone,'the exterior of the f urnac'e'is' ad-n ditionaly covered'with lheat insultation'"4| to insure retention of the heatof reaction. I In this form of retort, the carbon charge'i's 'supported on two plates '42 of semi-circularoutlinefresting on radial extensions I4 and retained inpositicn by guides I6 engaging notches 43 in plates' 42. The plates are apertured as at 424 andfrangible supports '4e (bricks,- ules or other mangime eiements) are positioned over the'aperture 4.4' to resumed by feeding carbon and sulfur,"
ve the charcoal charge support The space `ab is shown as including'a refractory liniigiBS; Such a liningfis desirablel to protect'the metashe'llin thereaction lzone inV either retort against corrof sion, for example, by the hot sulfur'vapo'rand yby various inorganic saltsor fother materials'pres--1 ent in -thel carbon source or added to the'"carbo' n source to improve the rate of reaction, as issugl gested in U.'S. Patent 2,026,840. 'Onlythe reacf tion zone proper need be-lined with asui'table rel fractoiygtc 'protect the metarsheug since heatis not'transferredthrough the shell wall injthe regio'nY of vthe lreaction' zone," adequateiprotection against corrosioncan be given in -thiszregion-by employing a'dense refractory, for exampl'ef'which is highly resistant to each V,of the various corrosive materials present.
Inthat form of `retort-,shown .iniFigures -5 and 6, the retort is provided with a plurality of #lugs 6I Y'at 'an elevation in "the tubular shell 4'8 iii's't above the sulfur inlet. Supported upon the lugs is a tubular shell 62 lhaving `several inwardly ex'- tending arms 53 'formed thereonfto rest upon each of the lugs i. The shell SZ-fand 'the shell '8 are "preferably cylindrical in shape fand cbncen# tric'ally positioned to provide a sulfur passage 'of uniform sectional size through which the sul-ful' ascends. The tubular shell 62 is provided with a conical upper 'end 6B. The shell 62 acts as a black -body or heat radiator in the upper portion of' thev tubular shell 8, to heat the sulfur passing between it and the 'shell 8 vby radiation whereby the sulfuris'raisd quien-lf.' toa reaction temperature.,
'The upper portion of the shell 3 and end "bell structure v26 includessuitabie refractory linings such asare indicated at "H and 12; that at 12 is particularly 'designed to be resistant to the car# bon-sulfur reaction because reaction 'occurs 'in this region, that is Where Vthe hot sulfur comes into contact with the carbon mass. Bell Y28 is preferably provided 'with a ange 'I3 at its upper end from which a tubular member 'i4' depends' in a spaced'relation to the heat refracting vlining?! to provide a passage to outlet 2,1 'so that'the carbon in the tubular member is out of the pathof the reaction products. Carbon is added through opening 15 upon raising of cover Tl With lever "This is a continuation-impart of my applicationv Serial N0. 40,512 filed July 24, 1948,' Anotti' abandoned. 5
I claim: t v
l. Apparatus for the manufacture of'carbon bisuliirieN comprising a furnace; an elongated tubular shellstandi'ng vertically in'said furnace andhaving a first inlet for feeding sulfur intoa lower portion of the vertical shell anda'second inlet for feeding carbon "into an upperpo'rtion of the vertical Shell; 'ra dical abutments intermediate the endso the shell; and s'upportmea'ns'resting on said abutment's and' extending transversely of the `shell and providing a support forv carbon fed into the shell KAthro'ughsaid second inlet, said support means dividing'th'e shell linto an upper reaction zone wherein'carbon and sulfur 'react and a' lower lzone wherein sulfurv admittedy tofgthe f lower' portion ofthel zo'ne is hea'jted to'a terni perature whereat the sulfur reacts withtle carbony to form carbonbisuiiide; atubular vessel provided in said elongated tubular shell below. said support' means andina spacedY relation toat least a'portion'of saidfeiongatedtubul i* shell' to prof videa passageway for Sulfur between a' portion ofthe inner'su'rface 'of said'shell'and the outer surface 'of said vessel, said tubular vvessel"havinga Jclosed conical topi an' outlet from "said" shell for products of reaction, rs'aid"`oi1t'ietbeingfiiioni said upper reaction'zone and communicating with the upper portion ci said sheli 'above said support means; said shell being" positioned inf said furnace with at least that portion of the shell defining thejs'ulfur heating' zone confined witiri'in andreceiving heat from"the`furnace.
' Apparatus "for the manufacture ofcarbon bisiifid'evv Comprising furnace; an emigrated JJJl'llit'l" "Shell Standing Vertitallyill` Sidlfuc' and havin'g'"a "first" inlet Vfor' feeding 'sulfur into' a lower portion of the vertical shell and a second inlet for feeding carbon into an upper portion of the vertical shell; radical abutments` intennediate the ends of the shell; support meansv resting on said abutments and extending transversely of the shell and providing a support for carbon fed into the shell through said second inlet, said support means dividing the shell into an upper reaction zone wherein carbon and sulfur react and a lower zone wherein sulfur admitted to the lower portion of the zone is heated by the furnace to a temperature whereat sulfur reacts with carbon to form carbon bisuliide; an elongated tubular vessel mounted in said tubular shell below said support means and spaced therefrom to provide a substantially uniform sulfur passage between said vessel and said shell, said tubular vessel having a closed conical top; an outlet from said shell for products of reaction,
said outlet being from said upper reaction zone i and communicating with the upper portion of said shell above said support means; said shell beingpositioned in said furnace with at least that portion of the shell defining the sulfur heating zone confined within and receiving heat from the furnace; and a refractory lining in said shell in that portion of the shell providing said reaction zone. l
3. Apparatus for the manufacture of carbon bisulde comprising a furnace; an elongated l tubular shell standing vertically in said furnace and having a first inlet for feeding sulfur into a lower portion of the vertical shell and a second inlet for feeding carbon into an upper portion of.. the vertical shell; radial abutments intermeg diate the ends of the shell; an elongated tubular vessel mounted in said tubular shell and spaced therefrom to provide a substantially uniform sulfur passage between said vessel and said shell, said tubular vessel having a closed conical top; and support means extending transversely of the shell over said tubular vesseland supported on said abutments and providingv a support for carbon fed into the shell through said second inlet, said support means dividing the shell into an upper reaction zone wherein carbon and sulfur react and a lower zone wherein sulfur admitted to the lower portion of the zone is heated by said furnace to a temperature whereafl the sulfur reacts with the carbon to form carbon bisuliide; a tubular deflector plate mounted above the support means on the vessel to deflect carbon from the passage between the vessel and the shell; an outlet from said shell for products of reaction, said outlet being from said upper reaction zone and communicating with the upper portion of said shell above said support means; said shell being positioned in said furnace with that portion of the shell defining the sulfur heating zone and at least a portion of the reaction zone confined within and receiving heat from the furnace.
4. Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace,
a first, inlet for feeding sulfur into a lower portion of the vertical shell, a second inlet forY feeding solid carbon particles into an upper portion of the vertical shell to provide a mass of carbon particles therein, an outlet from the upper portion of the shell for products of reaction; radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the, shell to divide the shell into an upper reaction v'zone containing said mass of carbon particles and wherein sulfur vapor and carbon react to form CS2 and leave a solid `ash residue and a lower zone which is heated bythe furnace and wherein sulfur admitted through said first inlet is, heated to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisuliide; said support means including a first carbon mass support including an annular grating shelf extending inwardly and transversely of the shell to provide a partial support for the carbon mass and to admit sulfur vapor into said upper reaction zone and having an opening therein through which the mass of carbon particles and ash residue in the reaction zone can fall freely into the lower zone, and a second carbon support including a temporary closure member mounted upon the grating shelf of the first carbon support over said opening normally to close said opening sufciently to retain said mass of carbon particles and ash residue in the upper zone, said second carbon support being movable to permit unreacted carbon and the ash residue to pass freely into the lower zone for removal from the tubular shell.
5. Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace, a first iniet for feeding sulfur into a lower portion of the vertical shell, a second inlet for feeding vsolid carbon particles into an upper portion n of the vertical shell to provide a mass of carbon particles therein, an outlet from the upper portion of the shell for products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell to divide the shell into an upper reaction zone containing said mass of carbon particles and wherein sulfur vapor and carbon react to form CS2 and leave a solid ash residue and a lower zone which is heated by the furnace and wherein sulfur admitted through said first inlet is heated to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisuliide; said support means including a iirsi-l carbon mass support including an annular grating shelf extending inwardly and transversely of the shell to provide a partial support for the carbon mass and having a plurality of openings therein to admit sulfur vapor into said upper reaction zone and through one of which openings the mass of carbon particles and ash residue in the reaction zone can fall freely into the lower zone, and a second carbon support including a temporary closure member mounted upon the grating shelf of the rst carbon support over said one opening normally to close said one opening and retain said mass of carbon particles in the upper zone and ash residue, said second carbon support being movable to drop unreacted carbon and the ash residue to pass freely into the lower zone for removal from the tubular shell.
6. Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace, a first inlet for feeding sulfur into a lower portion of the vertical shell in said furnace, a second inlet for feeding solid carbon particles into an upper portion of the vertical shell above said furnace to provide a mass of carbon particles therein, an outlet from the upper portion of the shellfor products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell at an elevation to divide the shell into. an upper reaction zone containing said mass of carbon particles and wherein sulfur and carbon react to form carbon bisulde and leave an ash residue and a lower zone wherein sulfur admitted through said rst inlet is heated as a vapor by said furnace to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisulde; said support means including carbon mass support including an annular grating shelf extending transversely of the shelf and having an opening therein through which the mass of carbon particles and any ash residue can pass to the lower zone, and at least one frangible support positioned on the grating shelf of said carbon mass support and extending across said opening normally to restrict said opening suciently to retain the mass of carbon particles and the ash residue in the upper zone and admit freely sulfur from the lower zone into contact with the mass of carbon in the upper zone, said frangible support being adapted to be broken with a poker extended down through said reaction zone to release the carbon charge and ash residue into the lower portion of the furnace for removal therefrom.
7. Apparatus for the manufacture of carbon bisulde comprising a furnace, an elongated tubular shell standing vertically in said furnace to receive heat therefrom in a lower portion, a rst inlet for feeding sulfur into a lower portion of the vertical shell, a second inlet for feeding solid carbon particles into an upper portion of the vertical shell to provide a mass of carbon particles therein, an outlet from the upper portion of the shell for products of reaction, radial abutments intermediate the ends of the shell, and support means resting on said abutments and extending transversely of the shell at an elevation to divide the shell into an upper reaction zone containing said massV of carbon particles and wherein sulfur and carbon react to form 10 carbon bisulde and leave an ash residue and a lower zone wherein sulfur admitted through said rst inlet is heated as a vapor to a temperature whereat the sulfur vapor is reactive with carbon to form carbon bisulde; said support means including carbon mass support including an annular grating shelf extending transversely of the shell and having an opening therein through which sulfur can pass from the lower zone and through which the mass of carbon particles and any ash residue can pass to the lower zone, and a plurality of frangible supports positioned on the grating shelf of said carbon mass support and extending across said opening in a spaced relation to one another and to the opening in said support normally to restrici-l said opening sufciently to retain the mass of carbon particles in the upper zone and admit freely sulfur from the lower zone into contact with the mass of carbon in the upper zone, said frangible supports being adapted to be broken with a poker extended down through said reaction zone to release the carbon charge and ash residue into the lower portion of the furnace for removal therefrom.
IVER C. MACDOUGALL.
REFERENCES CITED The following references are of record in the ile of this patent:
UNITED STATES PATENTS Number Name Date 321,661 Taylor July 7, 1884 605,812 Blackmore June 14, 1898 1,218,588 Barnett Mar. 6, 1917 1,705,614 Griswold Mar. 19, 1929 1,904,513 Nordlander Apr. 18, 1933 2,052,297 Iddings Aug. 25, 1936
Claims (1)
1. APPARATUS FOR THE MANUFACTURE OF CARBON BISULFIDE COMPRISING A FURNACE; AN ELONGATED TUBLULAR SHELL STANDING VERTICALLY IN SAID FURNACE AND HAVING A FIRST INLET FOR FEEDING SULFUR INTO A LOWER PORTION OF THE VERTICAL SHELL AND A SECOND INLET FOR FEEDING CARBON INTO AN UPPER PORTION OF THE VERTICAL SHELL; RADICAL ABUTMENTS INTERMEDIATE THE ENDS OF THE SHELL; AND SUPPORT MEANS RESTING ON SAID ABUTMENTS AND EXTENDING TRANSVERSELY OF THE SHELL AND PROVIDING A SUPPORT FOR CARBON FED INTO THE SHELL THROUGH SAID SECOND INLET, SAID SUPPORT MEANS DIVIDING THE SHELL INTO AN UPPER REACTION ZONE WHEREIN CARBON AND SULFUR REACT AND A LOWER ZONE WHEREIN SULFUR ADMITTED TO THE LOWER PORTION OF THE ZONE IS HEATED TO A TEMPERATURE WHEREAT THE SULFUR REACTS WITH THE CARBON TO FORM CARBON BISULFIED; A TUBULAR VESSEL PROVIDED IN SAID ELONGATED TUBULAR SHELL BELOW SAID SUPPORT MEANS AND IN A SPACED RELATION TO AT LEAST A PORTION OF SAID ELONGATED TUBULAR SHELL TO PROVIDE A PASSAGEWAY FOR SULFUR BETWEEN A PORTION OF THE INNER SURFACE OF SAID SHELL AND THE OUTER SURFACE OF SAID VESSEL, SAID TUBULAR VESSEL HAVING A CLOSED CONICAL TOP; AN OUTLET BEING FROM FOR PRODUCTS OF REACTIONS, SAID OUTLET BEING FROM SAID UPPER REACTION ZONE AND COMMUNICATING WITH THE UPPER PORTION OF SAID SHELL ABOVE SAID SUPPORT MEANS; SAID SHELL BEING POSITIONED IN SAID FURNACE WITH AT LEAST THAT PORTION OF HE SHELL DEFINING THE SULFUR HEATING ZONE CONFINED WITHIN AND RECEIVING HEAT FROM THE FURNACE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US162693A US2577786A (en) | 1950-05-18 | 1950-05-18 | Carbon bisulfide retort |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US162693A US2577786A (en) | 1950-05-18 | 1950-05-18 | Carbon bisulfide retort |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2577786A true US2577786A (en) | 1951-12-11 |
Family
ID=22586732
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US162693A Expired - Lifetime US2577786A (en) | 1950-05-18 | 1950-05-18 | Carbon bisulfide retort |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2577786A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2750264A (en) * | 1952-08-21 | 1956-06-12 | Stauffer Chemical Co | Carbon bisulfide retort |
| US3025144A (en) * | 1959-08-31 | 1962-03-13 | Stauffer Chemical Co | Carbon disulfide retort |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US321661A (en) * | 1885-07-07 | Apparatus for the manufacture of carbon bisulphide | ||
| US605812A (en) * | 1898-06-14 | Process of making aluminium sulfid | ||
| US1218588A (en) * | 1916-08-14 | 1917-03-06 | Alchlor Chemical Company | Art of producing aluminum chlorid. |
| US1705614A (en) * | 1927-01-27 | 1929-03-19 | Dow Chemical Co | Apparatus for chemical reaction on heated solid material |
| US1904513A (en) * | 1929-06-22 | 1933-04-18 | Gen Electric | Apparatus for preparing sulphur dioxide |
| US2052297A (en) * | 1933-10-18 | 1936-08-25 | Gen Chemical Corp | Carbon bisulphide process |
-
1950
- 1950-05-18 US US162693A patent/US2577786A/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US321661A (en) * | 1885-07-07 | Apparatus for the manufacture of carbon bisulphide | ||
| US605812A (en) * | 1898-06-14 | Process of making aluminium sulfid | ||
| US1218588A (en) * | 1916-08-14 | 1917-03-06 | Alchlor Chemical Company | Art of producing aluminum chlorid. |
| US1705614A (en) * | 1927-01-27 | 1929-03-19 | Dow Chemical Co | Apparatus for chemical reaction on heated solid material |
| US1904513A (en) * | 1929-06-22 | 1933-04-18 | Gen Electric | Apparatus for preparing sulphur dioxide |
| US2052297A (en) * | 1933-10-18 | 1936-08-25 | Gen Chemical Corp | Carbon bisulphide process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2750264A (en) * | 1952-08-21 | 1956-06-12 | Stauffer Chemical Co | Carbon bisulfide retort |
| US3025144A (en) * | 1959-08-31 | 1962-03-13 | Stauffer Chemical Co | Carbon disulfide retort |
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